Process of making homogeneous bodies from tantalum metal or other refractory metals.



' tion of metals like those here under considlifiill) STATES PATENT ()Fl liilfi.

\f RNER VOA ljUl/lON, Oi CllA RLOTTENBURG; GERMANY, A SSIGNOR TO Sllllt I"..\'.\' e; l l'AlS Kl", A KTIENGESELLSCHAFT, OF BERLIN, GERMANY.

PROCESS OF MAKING HOMOGENEOUS BODIES FROM TANTALUM METAL OR OTHER REFRACTORY METALS.

To all whom may concern:

Be it ltnown that I, VVERNER vox BOLTON, chemist, residing at Charlottenburg, near Berlin, Germany, 10 Liitzow, have invented a new and useful Process of Making Homogent-oils liodies from Tantalum Metal or other llct'ractory Metals, of which the following; is a'l'ull, clear, concise, and exact description.

In the treatment o'l' refractory metals, espci-iaii metals of the tantalum group, un- \Ollilllfih dilticultics are met with, it perfectly homogeneous bodies are to be made therei'rom. The drawing of said metals especially rendered highly difiicult, it we do not start with a quite homogeneous metallic material which can be obtained exclusively by a thorough melting process. However, tltt melting of such a metal constitutes a very ditlicult task, as the metal at the high lllt'llillg .emperaturcs is liable to enter into chemical combinations with the materials 01 its Filll'l'OllllkilllQS. ()u the other hand, it is by no mcaus easy to obtain suitable crucibles capable of withstanding the high temperatures utilized in the melting process.

Highly refractory materials, such, for instara-c, as tantalum and zirconium, or metals of kindred groups can be obtained in various w: but all processes known prior to the pro cnt time produce, as a result of their uscIa metal in the form of a powder. Met

ais in powdered form, however, cannot be used for a majority of purposes and par ticularly for the purpose of making firmly mhercnt bodies, as it is necessary to fuse such bodies into a coherent. or homogeneous in This melting or fusing is a comparatively simplev proc ss with easily melting or non rei'ractory metals, but in the producera! ion, which are very refractory, it has not been possible heretofore to produce homogeneous bodies; or, if it were possible to obtain such bedies'they were mixed to a very great extent with non-metallic impurities, such as carbids, etc, and, therefore, were useless for technical purposes.

My invention has for its objects, first, to offer or present a process of melting or fusing metals which have a very high melt ing point and which at high temperatures easily undergo chemical alterations when in Specification of Letters Patent.

Application filed January 5, 1904. Serial No. 187,830.

Patented Nov. 24:, 1908.

contact with other substances; and, second, to otler a process for melting metals of this nature into a homogeneous and pure metallic mass, and these results are eilected through the agency of an electric current which is conveyed through a compressed or united mass of metallic powder of the metal to be treated. For the purpose of practicing this method the metal powder might be used i111- mediatcly in the same sta'tc in which it is produced, but to do so would be very disadvantageous, for the reason that the loose powder of any metal offers an extremely variable resistance to an electric current. I, therefore, subject the powder of the metal to be treated to sullieient pressure to practically bind or unite it together or-gi ve to it a coherent or relatively solid mass and then pass a current of electricity through it, preferably while it is submerged in a rare atmosphere approximating a vacuum. For best cll'ecting this the mass of compressed powder is secured between clamps of tantalum con-- stituting the terminals of a source of electrical energy. The metal commences to fuse as soon as an electrical current of sutlicicut intensity is led hrough the compressed powder. The fusing process will generally proceed with relation to such compressed body of powder upon the principle that a small bar fuses at its thinnest point, or at the point of smallest cross section. and hence highest resistance. An arc is therefore formed at the "iusing point and in this are the further parts of the bar melt down, so that more or less large beads of molten metal'collect at the molten ends. These beads drop oil as the fusing proceeds.

Instead of forming a small bar of compressed metal powder and fusing it in the manner described, it will be preferable in most cases to press the metal powder into small rods'or similar bodies. These are placed on a plate of very refractory metal,

for instance, of tantalum, which forms one electrode, the other electrode being then approached to this body of compressed metal powder until both come into contact with each other. Thercupon the other electrode is somewhat removed again, whereby an arc formed in which the body of metal powder irradually melts. The molten body remains on the plate. It is also possible, of course,

to place a crucible below the molten metal to go on dropping into it as the fusin proceeds. 7

If the molten metal is brought into coir tact during the fusing process with other substances with which it is very liable to combine chemically at high temperatures,

the result will be a strongly impure product, i

and as almost all very refractory metals are most apt to chemically combine with other substances at the high tem eratures here in question, it is extremely di cult to obtain a pure metal. Above all, no carbon must be used as an electrode for fusing the metal, as otherwise the metal would take up too much carbon and might, under circumstances, be changed into a carbid. Further, all oxygen must be kept away and, therefore, all air must be pumped out of the fusing vessel as far as possible. Tantalum metal and many others are also liable to chemically combine with nitro en, hydrogen, etc., and, consequently, these injurious gases must also be kept away. Therefore, I prefer to axe cute the fusing process in a vacuum as perfeet as can be obtained and to have the electrodes between which the fusing takes place out of the same metal as that which is to be fused. 1 y

I have found that it is best to use direct current for the fusing process and to bring the metal to be fused-into contact with the positive electrode. This electrode may consist, for instance, of a small plate of the same metal as that which is to -be fused. The negative electrode may consist of another metal, as it will not so easily be broughtto fusing. ,aIf the negative electrode is large enou h it can be formed of pretty easily fusib e metals, such as silver, and will yet not combine with the molten product. Metallic bodies treated according to this process are the are and allow I quite homogeneous and have the highest degree of ductility which can be attained by the respective metals according to their chemical quality. Thus it is possible, without difficulty, to produce quite homogeneous bodies of tantalum metal. If pure raw material is used for the purpose and if all impurities process, the tantalum metal so obtained will have such a high degree of ductility that it can be rolled into very fine sheets and drawn into the finest of wires, while formerly it metal was quite brittle and could in no way be worked mechanically. Having thus described my invention what I claim and desireto secure by Letters Patent of the United States is- 1. A process of making homogeneous dies from tantalum or other1 highly refractory metals which consists in first compressing a quantity of the powder of the metal into a coherent mass; then heating the same to the melting or faising point through the agency of an electrical current and in an indifferent atmosphere. 4

2. A process of making homogeneous bodies from tantalum or other highly refractory metals which consists in uniting a powder of the metal into the form of a coherent mass; then heating said mass to the melting or fusing point by passing an electrical current through the same and simultaneously subjecting it to the action of a rare atmosphere.

-In witness whereof, I hereunto subscribe my name this 18th day of December A. 1).,

WERNER V. BOLTON. Witnesses:

HENRY HAsPER,

IVOLDEMAR HAUPT.

are kept away during the fusing was generally thought that pure tantalum 

